11-11-02 08:59
No 378719
Ok raf was trying to crash out some a-phenylacetoacetonitrile with acetic acid but accidentaly substituted acetic acid with formic acid.On the canister it was written Muurahaishappoa and i thoght it was acetic acid(raf's very bad in finnish).Well it's formic acid and no crystals crashed out.Is there anything he can do to save it or has he wasted few hundred bucks worth of chemicals and worked few weeks for nothing
,thanksA friend with speed is a friend indeed
(Chief Bee)
11-11-02 09:34
No 378725
It should be recoverable. Mix your solution with water and add aqueous sodium carbonate or bicarbonate with good stirring until no more carbon dioxide is given off to neutralize the acid, and then extract your nitrile with a nonpolar solvent, dry it over MgSO4 and evaporate the solvent to recover the nitrile in its original state.
(Hive Addict)
11-11-02 12:11
No 378750
Tried that,no results somehow.Anyway i'm not that frustrated,i still got lot of experience(and lots of empty reagent bottles).I did lose some money but what is money compared to experience and knownledge,right?.Next project for raf will be benzaldehyde to P2P.Anyway now i know i have about 15 liters of 85% technical formic acid and i'm sure it can be used for something.
Thanks Rhodium for lots of help(with this and with my other not so common experiments).
A friend with speed is a friend indeed
(Hive Addict)
11-11-02 13:32
No 378769
is this your first time?
if yes, then heat longer (4-6h) and stronger than what orgsyn says...
at least that's what some birds told me...
if no, then ignore... :)
(Chief Bee)
11-11-02 14:34
No 378794
raffike: Your product most definitely didn't vanish into thin air. It has to be there somewhere.
(Hive Addict)
11-11-02 22:01
No 378911
raffike: Your product most definitely didn't vanish into thin air. It has to be there somewhere.
Yeah,something went wrong during basifiyng and it might happened that thing didn't went over to NP.Or formic acid did something bad(not likely).
Anyway feel free to flame me as i screwed up just before P2P step.
A friend with speed is a friend indeed
(Hive Addict)
11-13-02 12:53
No 379369
what's fishy to me: it shouldn't make a difference
whether you use formic acid or acetic acid. after
all you're just neutralising an Na-Salt.
did you get the Na-Salt? did you wheigh it?
did you use anhydrous EtOH, freshly cut Na, and
did you reflux your EtAc over P2O5?
i've heard that this reaction works rather well if
anhydrous conditions are used. of course nowadays
you use a mag-stirrer...
